ASBESTOS IN AIR
Commercial manufacturers and products mentioned in this method are for descriptive use only and do
not constitute endorsements by
OSHA Technical Center Salt Lake City, Utah
1. Introduction This method describes the collection of airborne asbestos fibers using calibrated sampling pumps
with
Asbestos: A term for naturally occurring fibrous minerals. Asbestos includes chrysotile, crocidolite, amosite (cummingtonite-grunerite asbestos), tremolite asbestos, actinolite asbestos, anthophyllite asbestos, and any of these minerals that have been chemically treated and/or altered. The precise chemical formulation of each species will vary with the location from which it was mined. Nominal compositions are listed:
Asbestos Fiber: A fiber of asbestos which meets the criteria specified below for a fiber.
Early surveys to determine asbestos exposures were conducted using impinger counts of total dust with the counts expressed as million particles per cubic foot (8.1.). The British Asbestos Research Council (8.2.) recommended filter membrane counting in 1969. In July 1969, the Bureau of Occupational Safety and Health published a filter membrane method for counting asbestos fibers in the United States (8.3.). This method was refined by NIOSH and published as P & CAM 239 (8.4.). On May 29, 1971, OSHA specified filter membrane sampling with phase contrast counting for evaluation of asbestos exposures at work sites in the United States (8.5.). The use of this technique was again required by OSHA in 1986 (8.6.). Phase contrast microscopy has continued to be the method of choice for the measurement of occupational exposure to asbestos (8.7.). 1.2. Principle Air is drawn through a MCE filter to capture airborne asbestos fibers. A wedge shaped portion of the filter is removed, placed on a glass microscope slide and made transparent. A measured area (field) is viewed by PCM. All the fibers meeting defined criteria for asbestos are counted and considered a measure of the airborne asbestos concentration. 1.3. Advantages and Disadvantages There are four main advantages of PCM over other methods: 1) The technique is specific for fibers. Phase contrast is a fiber counting technique which
excludes 2) The technique is inexpensive and does not require specialized knowledge to carry out the analysis for total fiber counts. 3) The analysis is quick and can be performed 4) The technique has continuity with historical epidemiological studies so that estimates of
expected disease can be inferred from The main disadvantage of PCM is that it does not positively identify asbestos fibers. Other fibers which are not asbestos may be included in the count unless differential counting is performed. This requires a great deal of experience to adequately differentiate asbestos from non-asbestos fibers. Positive identification of asbestos must be performed by polarized light or electron microscopy techniques. A further disadvantage of PCM is that the smallest visible fibers are about 0.2 µm in diameter while the finest asbestos fibers may be as small as 0.02 µm in diameter. For some exposures, substantially more fibers may be present than are actually counted. 1.4. Workplace Exposure Asbestos is used by the construction industry in such products as shingles, floor tiles, asbestos
cement, roofing felts, insulation and acoustical products. About 95% of the asbestos in commercial use in the United States is chrysotile. Crocidolite and amosite make up most of the remainder. Anthophyllite and tremolite or actinolite are likely to be encountered as contaminants in various industrial products. 1.5. Physical Properties Asbestos fiber possesses a high tensile strength along its axis, is chemically inert, non-combustible, and heat resistant. It has a high electrical resistance and good sound absorbing properties. It can be weaved into cables, fabrics or other textiles, and also matted into asbestos papers, felts, or mats. 1.6. Toxic Effects
Information contained in this section is a synopsis of current knowledge of the physiological effects of asbestos and is not intended as a basis for OSHA policy.
2. Range and Detection Limit
2.2. The detection limit for this method is 4.0 fibers per 100 fields or 5.5 fibers/mm(2). This was determined using an equation to estimate the maximum CV possible at a specific concentration (95% confidence) and a Lower Control Limit of zero. The CV value was then used to determine a corresponding concentration from historical CV vs fiber relationships. As an example: Lower Control Limit (95% Confidence) = AC - 1.645(CV)(AC)
This value was compared with CV vs. count curves. The count at which CV = 0.61 for
Leidel-Busch counting statistics (8.9.) or for an OSHA Salt Lake Technical Center
(OSHA-SLTC) CV curve (see Appendix A for further information) was 4.4 fibers or 3.9 fibers
per 100 fields, respectively. Although a lower detection limit of 4 fibers per 100 fields is
supported by the 3. Method Performance - Precision and Accuracy Precision is dependent upon the total number of fibers counted and the uniformity of the fiber distribution on the filter. A general rule is to count at least 20 and not more than 100 fields. The count is discontinued when 100 fibers are counted, provided that 20 fields have already been counted. Counting more than 100 fibers results in only a small gain in precision. As the total count drops below 10 fibers, an accelerated loss of precision is noted (8.9.). At this time, there is no known method to determine the absolute accuracy of the asbestos
analysis. Results of samples prepared through the Proficiency Analytical Testing (PAT) Program
and analyzed by the 4. Interferences Fibrous substances, if present, may interfere with asbestos analysis. Some common fibers are:
The use of electron microscopy or optical tests such as polarized light, and dispersion staining may be used to differentiate these materials from asbestos when necessary. 5. Sampling
Conductive filter holder consisting of a
5.1.3 Sampling pump: Each pump must be a battery operated, 5.1.4. Flexible tubing, 5.1.5. Pump calibration: Stopwatch and bubble tube/burette or electronic meter. 5.2. Sampling Procedure
5.2.2. Charge the pumps completely before beginning. 5.2.3. Connect each pump to a calibration cassette with an appropriate length of 5.2.4. Select an appropriate flow rate for the situation being monitored. The sampling flow rate must be between 0.5 and 5.0 L/min for personal sampling and is commonly set between 1 and 2 L/min. Always choose a flow rate that will not produce overloaded filters. 5.2.5. Calibrate each sampling pump before and after sampling with a calibration cassette in-line (Note: This calibration cassette should be from the same lot of cassettes used for sampling). Use a primary standard (e.g. bubble burette) to calibrate each pump. If possible, calibrate at the sampling site.
5.2.7. A suggested minimum air volume when sampling to determine TWA compliance is 25 L. For Excursion Limit (30 min sampling time) evaluations, a minimum air volume of 48 L is recommended. 5.2.8. The most significant problem when sampling for asbestos is overloading the filter with non-asbestos dust. Suggested maximum air sample volumes for specific environments are:
Do not overload the filter with dust. High levels of
5.2.9. Blank samples are used to determine if any contamination has occurred during sample handling. Prepare two blanks for the first 1 to 20 samples. For sets containing greater than 20 samples, prepare blanks as 10% of the samples. Handle blank samples in the same manner as air samples with one exception: Do not draw any air through the blank samples. Open the blank cassette in the place where the sample cassettes are mounted on the employee. Hold it open for about 30 seconds. Close and seal the cassette appropriately. Store blanks for shipment with the sample cassettes. 5.2.10. Immediately after sampling, close and seal each cassette with the base and plastic plugs. Do not touch or puncture the filter membrane as this will invalidate the analysis. 5.2.11. Attach a seal (OSHA-21 or equivalent) around each cassette in such a way as to
secure the end cap plug and base plug. Tape the ends of the seal together since the
seal is not long enough to be wrapped 5.3. Sample Shipment 5.3.1. Send the samples to the laboratory with paperwork requesting asbestos analysis. List any known fibrous interferences present during sampling on the paperwork. Also, note the workplace operation(s) sampled. 5.3.2. Secure and handle the samples so that they will not rattle during shipment nor be exposed to static electricity. Do not ship samples in expanded polystyrene peanuts, vermiculite, paper shreds, or excelsior. Tape sample cassettes to sheet bubbles and place in a container that will cushion the samples without rattling. 5.3.3. To avoid the possibility of sample contamination, always ship bulk samples in separate mailing containers. 6. Analysis
6.1.2. Any asbestos spills should be cleaned up immediately to prevent dispersal of fibers.
Prudence should be exercised to avoid contamination of laboratory facilities or
exposure of personnel to asbestos. Asbestos spills should be cleaned up with wet
methods and/or a High Efficiency 6.2. Equipment
6.2.2. Widefield or Huygenian 10X eyepieces (NOTE: The eyepiece containing the graticule must be a focusing eyepiece. Use a 40X phase objective with a numerical aperture of 0.65 to 0.75). 6.2.3. Kohler illumination (if possible) with green or blue filter. 6.2.4. 6.2.5. Mechanical stage. A rotating mechanical stage is convenient for use with polarized light. 6.2.6. Phase telescope. 6.2.7. Stage micrometer with 0.01-mm subdivisions. 6.2.8. 6.2.9. Precleaned glass slides, 25 mm X 75 mm. One end can be frosted for convenience in
writing sample numbers, etc., or 6.2.10. Cover glass #1½. 6.2.11. Scalpel (#10, curved blade). 6.2.12. Fine tipped forceps. 6.2.13. Aluminum block for clearing filter (see Appendix D and Figure 4). 6.2.14. Automatic adjustable pipette, 6.2.15. Micropipette, 5 µL. 6.3. Reagents
6.3.2. Triacetin (glycerol triacetate). 6.3.3. Lacquer or nail polish. 6.4. Standard Preparation A way to prepare standard asbestos samples of known concentration has not been developed. It is possible to prepare replicate samples of nearly equal concentration. This has been performed through the PAT program. These asbestos samples are distributed by the AIHA to participating laboratories. Since only about 6.5. Sample Mounting
An aluminum block or similar device is required for sample preparation. A drawing is shown in Figure 4.
6.5.2. Ensure that the glass slides and cover glasses are free of dust and fibers. 6.5.3. Remove the top plug to prevent a vacuum when the cassette is opened. Clean the outside of the cassette if necessary. Cut the seal and/or tape on the cassette with a razor blade. Very carefully separate the base from the extension cowl, leaving the filter and backup pad in the base. 6.5.4. With a rocking motion cut a triangular wedge from the filter using the scalpel. This
wedge should be 6.5.5. Place the tip of the micropipette containing about 200 µL acetone into the aluminum block. Insert the glass slide into the receiving slot in the aluminum block. Inject the acetone into the block with slow, steady pressure on the plunger while holding the pipette firmly in place. Wait 3 to 5 seconds for the filter to clear, then remove the pipette and slide from the aluminum block. 6.5.6. Immediately (less than 30 seconds) place 2.5 to 3.5 µL of triacetin on the filter (NOTE: Waiting longer than 30 seconds will result in increased index of refraction and decreased contrast between the fibers and the preparation. This may also lead to separation of the cover slip from the slide). 6.5.7. Lower a cover slip gently onto the filter at a slight angle to reduce the possibility of forming air bubbles. If more than 30 seconds have elapsed between acetone exposure and triacetin application, glue the edges of the cover slip to the slide with lacquer or nail polish. 6.5.8. If clearing is slow, warm the slide for 15 min on a hot plate having a surface temperature of about 50°C to hasten clearing. The top of the hot block can be used if the slide is not heated too long. 6.5.9. Counting may proceed immediately after clearing and mounting are completed. 6.6. Sample Analysis Completely align the microscope according to the manufacturer's instructions. Then, align the microscope using the following general alignment routine at the beginning of every counting session and more often if necessary. 6.6.1. Alignment 1) Clean all optical surfaces. Even a small amount of dirt can significantly degrade the image. 2) Rough focus the objective on a sample. 3) Close down the field iris so that it is visible in the field of view. Focus the image of the iris with the condenser focus. Center the image of the iris in the field of view. 4) Install the phase telescope and focus on the phase rings. Critically center the rings. Misalignment of the rings results in astigmatism which will degrade the image. 5) Place the 6.6.2. Counting Fibers 1) Place the prepared sample slide on the mechanical stage of the microscope. Position the center of the wedge under the objective lens and focus upon the sample. 2) Start counting from one end of the wedge and progress along a radial line to the other end (count in either direction from perimeter to wedge tip). Select fields randomly, without looking into the eyepieces, by slightly advancing the slide in one direction with the mechanical stage control. 3) Continually scan over a range of focal planes (generally the upper 10 to 15 µm of the filter surface) with the fine focus control during each field count. Spend at least 5 to 15 seconds per field. 4) Most samples will contain asbestos fibers with fiber diameters less than 1 µm. Look carefully for faint fiber images. The small diameter fibers will be very hard to see. However, they are an important contribution to the total count. 5) Count only fibers equal to or longer than 5 µm. Measure the length of curved fibers along the curve. 6) Count fibers which have a length to width ratio of 3:1 or greater. 7) Count all the fibers in at least 20 fields. Continue counting until either 100 fibers are counted or 100 fields have been viewed; whichever occurs first. Count all the fibers in the final field. 8) Fibers lying entirely within the boundary of the 9) Count bundles of fibers as one fiber unless individual fibers can be clearly identified and each individual fiber is clearly not connected to another counted fiber. See Figure 2 for counting conventions. 10) Record the number of fibers in each field in a consistent way such that filter non-uniformity can be assessed. 11) Regularly check phase ring alignment. 12) When an agglomerate (mass of material) covers more than 25% of the field of view, reject the field and select another. Do not include it in the number of fields counted. 13) Perform a "blind recount" of 1 in every 10 filter wedges (slides). 6.7. Fiber Identification As previously mentioned in Section 1.3., PCM does not provide positive confirmation of asbestos fibers. Alternate differential counting techniques should be used if discrimination is desirable. Differential counting may include primary discrimination based on morphology, polarized light analysis of fibers, or modification of PCM data by Scanning Electron or Transmission Electron Microscopy. A great deal of experience is required to routinely and correctly perform differential counting. It is discouraged unless it is legally necessary. Then, only if a fiber is obviously not asbestos should it be excluded from the count. Further discussion of this technique can be found in reference 8.10.
"WHEN IN DOUBT, COUNT."
6.8.1. All individuals performing asbestos analysis must have taken the NIOSH course for sampling and evaluating airborne asbestos or an equivalent course. 6.8.2. Each laboratory engaged in asbestos counting shall set up a slide trading arrangement with at least two other laboratories in order to compare performance and eliminate inbreeding of error. The slide exchange occurs at least semiannually. The round robin results shall be posted where all analysts can view individual analyst's results. 6.8.3. Each laboratory engaged in asbestos counting shall participate in the Proficiency Analytical Testing Program, the Asbestos Analyst Registry or equivalent. 6.8.4. Each analyst shall select and count prepared slides from a "slide bank". These are quality assurance counts. The slide bank shall be prepared using uniformly distributed samples taken from the workload. Fiber densities should cover the entire range routinely analyzed by the laboratory. These slides are counted blind by all counters to establish an original standard deviation. This historical distribution is compared with the quality assurance counts. A counter must have 95% of all quality control samples counted within three standard deviations of the historical mean. This count is then integrated into a new historical mean and standard deviation for the slide. The analyses done by the counters to establish the slide bank may be used for an interim quality control program if the data are treated in a proper statistical fashion. 7. Calculations
where: AC = Airborne fiber concentration FB = Total number of fibers greater than 5 µm counted FL = Total number of fields counted on the filter BFB = Total number of fibers greater than 5 µm counted in the blank BFL = Total number of fields counted on the blank ECA = Effective collecting area of filter (385 mm(2) nominal for a FR = Pump flow rate (L/min) MFA = Microscope count field area (mm(2)). This is 0.00785 mm(2) for a T = Sample collection time (min) 1,000 = Conversion of L to cc
Since a given analyst always has the same interpupillary distance, the number of fields per filter for a particular analyst will remain constant for a given size filter. The field size for that analyst is constant (i.e. the analyst is using an assigned microscope and is not changing the reticle). For example, if the exposed area of the filter is always 385 mm(2) and the size of the field is always 0.00785 mm(2), the number of fields per filter will always be 49,000. In addition it is necessary to convert liters of air to cc. These three constants can then be combined such that ECA/(1,000 X MFA) = 49. The previous equation simplifies to:
7.3. Recount Calculations As mentioned in step 13 of Section 6.6.2., a "blind recount" of 10% of the slides is performed. In all cases, differences will be observed between the first and second counts of the same filter wedge. Most of these differences will be due to chance alone, that is, due to the random variability (precision) of the count method. Statistical recount criteria enables one to decide whether observed differences can be explained due to chance alone or are probably due to systematic differences between analysts, microscopes, or other biasing factors. The following recount criterion is for a pair of counts that estimate AC in fibers/cc. The
criterion is given at the
Reject a pair of counts if:
AC(1) = lower estimated airborne fiber concentration AC(2) = higher estimated airborne fiber concentration CV(FB) = Pooled average CV for the two concentration estimates:
CV(1) = Coefficient of variation associated with the lower count
Coefficients of variation (CV) may be determined as in Appendix A of this method (ID-160) or as
discussed in NIOSH Method 7400.
7.4. Reporting Results Report results to the industrial hygienist as fibers/cc. Use two significant figures. If multiple analyses are performed on a sample, an average of the results is to be reported unless any of the results can be rejected for cause. 8. References
8.2. Asbestos Research Council: The Measurement of Airborne Asbestos Dust by the Membrane Filter Method (Technical Note), Asbestos Research Council, Rockdale, Lancashire, Great Britain, 1969. 8.3. Bayer, S.G., Zumwalde, R.D., Brown, T.A., Equipment and Procedure for Mounting Millipore Filters and Counting Asbestos Fibers by Phase Contrast Microscopy, Bureau of Occupational Health, U.S. Dept. of Health, Education and Welfare, Cincinnati,OH,1969.
8.4. NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1 (DHEW/NIOSH Pub. No. 8.5. Asbestos, Code of Federal Regulations 29 CFR 1910.1001. 1971.
8.6. Occupational Exposure to Asbestos, Tremolite, Anthophyllite, and Actinolite. Final Rule,
Federal Register 51: 119 (20 June 1986).
8.7. Asbestos, Tremolite, Anthophyllite, and Actinolite, Code of Federal Regulations 1910.1001.
1988.
8.8. Criteria for a Recommended Standard -- Occupational Exposure to Asbestos (DHEW/NIOSH
Pub. No. HSM
8.9. Leidel, N.A., Bayer,S.G., Zumwalde, R.D.,Busch, K.A., USPHS/NIOSH Membrane Filter
Method for Evaluating Airborne Asbestos Fibers (DHEW/NIOSH Pub. No.
8.10. Dixon, W.C., Applications of Optical Microscopy in Analysis of Asbestos and Quartz,
Analytical Techniques in Occupational Health Chemistry, edited by D.D. Dollberg and A.W.
Verstuyft. Wash. D.C.: American Chemical Society, (ACS Symposium Series 120) 1980. pp.
8.11. Abell, M. T., et al.,The Quality of Fiber Count Data, Appl. Ind. Hyg. Vol 4 No.11,
November 1989, pp. Appendix A
The OSHA asbestos regulations require each laboratory to establish a quality control program. The
following is presented as an example of how the Data for the CV curve shown below is from 395 samples collected during OSHA compliance inspections and analyzed from October 1980 through April 1986. Each sample was counted by 2 to 5 different counters independently of one another. The standard deviation and the CV statistic was calculated for each sample. This data was then plotted on a graph of CV vs. fibers/mm(2). A least squares regression was performed using the following equation:
Application of least squares gave:
B = -0.973343 C = 0.327499 Using these values, the equation becomes: CV = antilog(10)[0.182205(log(10)(x))(2) - 0.973343(log(10)(x)) + 0.327499]
Appendix B Sampling Pump Flow Rate Corrections This correction is used if a difference greater than 5% in ambient temperature and/or pressure is noted
between calibration and sampling sites and the pump does not compensate for the differences.
Where:
Q(cal) = calibrated flow rate (if a rotameter was used, the rotameter value) P(cal) = uncorrected air pressure at calibration P(act) = uncorrected air pressure at sampling site T(act) = temperature at sampling site (K) T(cal) = temperature at calibration (K) Walton-Beckett Graticule When ordering the Graticule for asbestos counting, specify the exact disc diameter needed to fit the ocular of the microscope and the diameter (mm) of the circular counting area. Instructions for measuring the dimensions necessary are listed:
The Graticule is available from: Graticules Ltd., Morley Road, Tonbridge TN9 IRN, Kent, England
(Telephone Appendix D Aluminum Block Diagrams of the block are provided in Figure 4. The cartridge thermostat and heater used for this block have the following dimensions:
These heating units were obtained from:
Kezar Falls, Maine 04047 (207)-625-3231
Figure 3: Walton-Beckett Graticule with some explanatory fibers. Counts for the fibers in the figure
Figure 4: Engineering Drawings for the aluminum "Hot Block" as used at the Salt Lake Technical Center.
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